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Simultaneous determination of carisoprodol and meprobamate in human hair using solid-phase extraction and gas chromatography/mass spectrometry of the trimethylsilyl derivatives.
Rapid Commun Mass Spectrom. 2005; 19(21):3056-62.RC

Abstract

Carisoprodol (CSP) is a musculoskeletal relaxant whose active metabolite is meprobamate (MPB). This drug has recently been noticed to be abused as an inexpensive alternative to illicit drugs in Korea. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of CSP and MPB in human hair. Hair samples (30 mg) were washed with distilled water and acetone, cut into small fragments (<1 mm), incubated in 1.0 M HCl overnight at 50 degrees C, and then adjusted to pH 6.5. The drugs were extracted from the resulting hydrolyzed solutions using a SPE column. The eluents were evaporated to dryness, then derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) at 120 degrees C for 30 min. The derivatized extract (1 microL) was injected into the GC/MS system. Recoveries were in the range of 91.5-93.1% for CSP and 85.5-93.0% for MPB. The linear ranges were 0.5-10.0 ng/mg for both CSP and MPB with good correlation coefficients (r(2) = 0.995). The intra-day precision and accuracy ranged from 1.5 to 9.3% and -17.5 to 3.6%, respectively, and the inter-day precision and accuracy ranged from 3.9 to 6.2% and -15.0 to -3.9%, respectively. The limits of detection for CSP and MPB were 0.13 and 0.12 ng/mg, respectively. The applicability of the method was proven by analyzing a hair sample from an authentic abuser.

Authors+Show Affiliations

Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seoul, Korea.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Journal Article
Validation Study

Language

eng

PubMed ID

16200657

Citation

Kim, Jin Young, et al. "Simultaneous Determination of Carisoprodol and Meprobamate in Human Hair Using Solid-phase Extraction and Gas Chromatography/mass Spectrometry of the Trimethylsilyl Derivatives." Rapid Communications in Mass Spectrometry : RCM, vol. 19, no. 21, 2005, pp. 3056-62.
Kim JY, In MK, Paeng KJ, et al. Simultaneous determination of carisoprodol and meprobamate in human hair using solid-phase extraction and gas chromatography/mass spectrometry of the trimethylsilyl derivatives. Rapid Commun Mass Spectrom. 2005;19(21):3056-62.
Kim, J. Y., In, M. K., Paeng, K. J., & Chung, B. C. (2005). Simultaneous determination of carisoprodol and meprobamate in human hair using solid-phase extraction and gas chromatography/mass spectrometry of the trimethylsilyl derivatives. Rapid Communications in Mass Spectrometry : RCM, 19(21), 3056-62.
Kim JY, et al. Simultaneous Determination of Carisoprodol and Meprobamate in Human Hair Using Solid-phase Extraction and Gas Chromatography/mass Spectrometry of the Trimethylsilyl Derivatives. Rapid Commun Mass Spectrom. 2005;19(21):3056-62. PubMed PMID: 16200657.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of carisoprodol and meprobamate in human hair using solid-phase extraction and gas chromatography/mass spectrometry of the trimethylsilyl derivatives. AU - Kim,Jin Young, AU - In,Moon Kyo, AU - Paeng,Ki-Jung, AU - Chung,Bong Chul, PY - 2005/10/4/pubmed PY - 2005/12/15/medline PY - 2005/10/4/entrez SP - 3056 EP - 62 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 19 IS - 21 N2 - Carisoprodol (CSP) is a musculoskeletal relaxant whose active metabolite is meprobamate (MPB). This drug has recently been noticed to be abused as an inexpensive alternative to illicit drugs in Korea. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of CSP and MPB in human hair. Hair samples (30 mg) were washed with distilled water and acetone, cut into small fragments (<1 mm), incubated in 1.0 M HCl overnight at 50 degrees C, and then adjusted to pH 6.5. The drugs were extracted from the resulting hydrolyzed solutions using a SPE column. The eluents were evaporated to dryness, then derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) at 120 degrees C for 30 min. The derivatized extract (1 microL) was injected into the GC/MS system. Recoveries were in the range of 91.5-93.1% for CSP and 85.5-93.0% for MPB. The linear ranges were 0.5-10.0 ng/mg for both CSP and MPB with good correlation coefficients (r(2) = 0.995). The intra-day precision and accuracy ranged from 1.5 to 9.3% and -17.5 to 3.6%, respectively, and the inter-day precision and accuracy ranged from 3.9 to 6.2% and -15.0 to -3.9%, respectively. The limits of detection for CSP and MPB were 0.13 and 0.12 ng/mg, respectively. The applicability of the method was proven by analyzing a hair sample from an authentic abuser. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/16200657/Simultaneous_determination_of_carisoprodol_and_meprobamate_in_human_hair_using_solid_phase_extraction_and_gas_chromatography/mass_spectrometry_of_the_trimethylsilyl_derivatives_ L2 - https://doi.org/10.1002/rcm.2173 DB - PRIME DP - Unbound Medicine ER -